中藥製劑中摻加Fluoxymesterone, Methyltestosterone及Testosterone之高效液相層析法定量探討   全文下載

Determination by High Performance Liquid Chromatography of Fluoxymesterone, Methyltestosterone and Testosterone in Adulterated Chinese Herbal Preparations

本研究利用高效液相層析方法，分析添加於中藥製劑之三種fluoxymesterone、methyltestosterone及testosterone男性荷爾蒙成分之可行性。本方法採用C18逆相層析管柱，以水：乙?（3 : 2）沖提。結果顯示，三種西藥成分之檢量線於10~160μg／ml濃度之線性相關係數介於0.9997至0.9999間，顯示良好之線性關係。模擬添加於八珍湯之回收率依序為fluoxymesterone 87.7%；methyltestosterone 99.3%；及testosterone 91.1%，顯示準確性尚可接受。最低檢出濃度介於0.05μg／ml至0.10μg／ml間。同日內及異日間之相對標準差分別為0.31~ 2.01%，0.95~ 5.11%，顯示再現性亦可接受。依此方法分析本局受理檢驗之四種自稱為?鞭、蛇鞭膠囊中檢出methyltestosterone之情況，其添加回收率分別為95.4、83.3、92.7及88.8%。至於該四種膠囊所含methyltestosterone之量介於1.5~4.0%之間。換算成單位含量則12粒膠囊檢體中每粒methyltestosterone之含量介於7.5 mg至19.7 mg之間。 A Chinese herbal preparation was assayed simultaneously by high performance liquid chromatography on an ODS column for the presence of adulterated three androgens, fluoxymesterone, methyltestosterone and testosterone. This chromatographic method was carried out using isocratic elution with water and acetonitrile (3:2). Calibration graphs of the three adulterants were constructed in the range 10-160 μg/ml and their correlation coefficients were in the range 0.9997-0.9999. When these three androgens were added to Ba-Jen-Tang, the recoveries were 87.7 % for fluoxymesterone, 99.3% for methyltestosterone and 91.1 % for testosterone. The relative standard deviations for intraday and interday analyses were 0.31-2.01 % and 0.95-5.11 % (n=6), respectively. Four kinds of capsules labeled snake penis (Samples A-D) were consigned during Aug. 1995 and Jul. 1996. The methyltestosterone in the samples was assayed by the HPLC method described above. The recoveries of methyltestosterone in samples A, B, C and D were 95.4, 83.3, 92.7 and 88.8%, respectively. The content of methyltestosterone in these capsules ranged from 1.5 to 4.0% (7.5-19.7 mg in each capsule). Caffeine, diprophylline and three water soluble vitamins (ascorbic acid, nicotinamide and thiamine) were also detected in Samples A and B, and thiamine was detected in Samples C and D. The identity of these chemicals was confirmed by TLC and UV."

A Chinese herbal preparation was assayed simultaneously by high performance liquid chromatography on an ODS column for the presence of adulterated three androgens, fluoxymesterone, methyltestosterone and testosterone. This chromatographic method was carried out using isocratic elution with water and acetonitrile (3:2). Calibration graphs of the three adulterants were constructed in the range 10-160 µg/ml and their correlation coefficients were in the range 0.9997-0.9999. When these three androgens were added to Ba-Jen-Tang, the recoveries were 87.7 % for fluoxymesterone, 99.3% for methyltestosterone and 91.1 % for testosterone. The relative standard deviations for intraday and interday analyses were 0.31-2.01 % and 0.95-5.11 % (n=6), respectively. Four kinds of capsules labeled snake penis (Samples A-D) were consigned during Aug. 1995 and Jul. 1996. The methyltestosterone in the samples was assayed by the HPLC method described above. The recoveries of methyltestosterone in samples A, B, C and D were 95.4, 83.3, 92.7 and 88.8%, respectively. The content of methyltestosterone in these capsules ranged from 1.5 to 4.0% (7.5-19.7 mg in each capsule). Caffeine, diprophylline and three water soluble vitamins (ascorbic acid, nicotinamide and thiamine) were also detected in Samples A and B, and thiamine was detected in Samples C and D. The identity of these chemicals was confirmed by TLC and UV.